CN102636931A - Electro-chromic layer, coated element and preparation method of coated element - Google Patents
Electro-chromic layer, coated element and preparation method of coated elementDownload PDFInfo
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- CN102636931A CN102636931ACN2011100384845ACN201110038484ACN102636931ACN 102636931 ACN102636931 ACN 102636931ACN 2011100384845 ACN2011100384845 ACN 2011100384845ACN 201110038484 ACN201110038484 ACN 201110038484ACN 102636931 ACN102636931 ACN 102636931A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
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Abstract
Description
Technical field
The present invention relates to a kind of electrochromic layer, have the preparation method of plated film spare and this plated film spare of this electrochromic layer.
Background technology
Electrochromic material is under impressed voltage or effect of electric field, and reversible variation can take place for the color of material or transparency.When voltage that adds or electric field disappearance, the color or the transparency of material return back to original state.Electrochomeric films has memory function, is widely used in fields such as display device, dimming glass, information stores and decorative appearance.Existing plated film spare with colour change function comprises base material and is formed at the electrochomeric films on the base material that said electrochomeric films generally includes first transparency conducting layer, electrochromic layer, ion conductive layer, ion storage and second transparency conducting layer that stacks gradually.This first and second transparency conducting layer is used to apply electric field, and under the effect of extra electric field, the ion in said ion conductive layer and the ion storage gets into electrochromic layer, said electrochromic layer generation redox reaction, thus color changes.
Mostly existing electrochromic layer is that the organic electrochromic material processes.Redox reaction takes place in the organic electrochromic material under effect of electric field, the light absorption transmitance of electrochomeric films is changed and color is changed.Yet the reversibility of organic electrochromic material is relatively poor, causes in the process that this electrochromic layer uses unstablely, and serviceable life is shorter.
Summary of the invention
In view of this, be necessary to provide a kind of stable height and serviceable life long electrochromic layer.
Also be necessary to provide a kind of plated film spare with above-mentioned electrochromic layer.
In addition, also be necessary to provide a kind of preparation method of above-mentioned plated film spare.
A kind of electrochromic layer; This electrochromic layer is the tungsten oxide layer that A mixes; Wherein A is one or more in molybdenum, niobium and the titanium, and in this electrochromic layer, the A atomic percentage conc is 4～12%; The variable color voltage of this electrochromic layer is 2.1～2.8V, and said electrochromism layer thickness is 500～800nm.
A kind of plated film spare comprises electrochromic layer, and this electrochromic layer is the tungsten oxide layer that A mixes; Wherein A is one or more in molybdenum, niobium and the titanium; In this electrochromic layer, the atomic percentage conc of A is 4～12%, and the variable color voltage of this electrochromic layer is 2.1～2.8V.
A kind of preparation method of plated film spare may further comprise the steps:
The base material, vacuum coating equipment and the alloy target material that have transparency conducting layer are provided, and this alloy target material is the tungsten of doping A, and A is at least a in molybdenum, niobium and the titanium, and the A atomic percentage conc is 5～15%;
Base material and alloy target material are installed in the vacuum coating equipment;
Aerating oxygen, plated film forms electrochromic layer on base material, and the variable color voltage of this electrochromic layer is 2.1～2.8V.
Electrochromic layer of the present invention adopts the tungsten oxide of doping A to process, and this tungsten oxide applies electric field and removes in the process of electric field, has good reversibility, can improve the serviceable life of electrochromic layer effectively.
Description of drawings
Fig. 1 is the cut-open view of the present invention's one preferred embodiment plated film spare;
Fig. 2 is the synoptic diagram of the present invention's one preferred embodiment vacuum coating equipment.
The main element symbol description
Plated film spare 10
Firsttransparency conducting layer 12
Ionconductor layer 14
Ion storage 15
Secondtransparency conducting layer 16
Coatingchamber 21
Alloytarget material 23
Embodiment
See also Fig. 1, the plated film spare of preferred embodiments of thepresent invention 10, it comprisesbase material 11 and firsttransparency conducting layer 12,electrochromic layer 13,ion conductor layer 14, ion storage 15 and secondtransparency conducting layer 16 that stack gradually.Said firsttransparency conducting layer 12 and secondtransparency conducting layer 16 are used for this platedfilm spare 10 is applied electric field, make it to take place variable color.Thision conductor layer 14 and ion storage 15 are used under the effect of extra electric field, for thiselectrochromic layer 13 electronics and ion being provided, and makeelectrochromic layer 13 redox reaction take place and variable color.
This firsttransparency conducting layer 12 is that (Indiumtin oxide, ITO) or aluminum zinc oxide transparent conductive film (AZO), it can adopt sputter or vapor deposition indium tin oxide or aluminum zinc oxide to form to indium tin oxide transparent conductive semiconductor film.
Thision conductor layer 14 is by LiTaO3Or LiNbO3Form through the collosol and gel mode.
This ion storage 15 is by V2O5, NiOxDeng forming through sputter or collosol and gel mode.
This secondtransparency conducting layer 16 is indium tin oxide transparent conductive semiconductor film or aluminum zinc oxide transparent conductive film glass, and it can adopt the mode of sputter or vapor deposition to form.
(wolframium oxide, the symbol of element are WO to the tungsten oxide that thiselectrochromic layer 13 mixes for A3), wherein A can be one or more in molybdenum (molybdnum, the symbol of element are Mo), niobium (niobium, the symbol of element are Nb), the titanium (titanium, the symbol of element are Ti); The A atomic percentage conc is 4～12% in thiselectrochromic layer 13, and the thickness of thiselectrochromic layer 13 can be 500～800nm, and its variable color voltage is 2.1～2.8V.Saidelectrochromic layer 13 can adopt the mode of magnetron sputtering to form.A behind the said doped with tungstic oxide, because the atomic radius of A radius and tungsten is close, the growing up of inhibition tungsten oxide crystal grain when forming electrochromic layer, grain refinement has increased the access way of ion.In addition, because the existence of A destroys part W-O-W key, under the effect of extra electric field, more help the turnover of ion, thereby reduced critical variable color voltage.This tungsten oxide applies electric field and removes in the process of electric field, has good reversibility, has improved the stability ofelectrochromic layer 13, thereby has improved its serviceable life.
The material of thisbase material 11 can be stainless steel, aluminium alloy, magnesium alloy, glass, pottery or plastics.
The preparation method of the plated film spare of preferred embodiments of thepresent invention 10 mainly comprises the steps:
Adopt sputter or vapor deposition indium tin oxide or aluminum zinc oxide onbase material 11, to form said firsttransparency conducting layer 12.
Adopt magnetron sputtering method on firsttransparency conducting layer 12, to form said electrochromic layer 13 (will combine accompanying drawing 2 to specify).Onelectrochromic layer 13, formion conductor layer 14 through the collosol and gel mode.
Form said ion storage 15 through sputter or collosol and gel mode.
Adopt sputter or vapor deposition indium tin oxide or aluminum zinc oxide onbase material 11, to form said firsttransparency conducting layer 12.
See also Fig. 2, thebase material 11,vacuum coating equipment 20 and thealloy target material 23 that have transparency conducting layer are provided, thisbase material 11 is processed by stainless steel, aluminium alloy, magnesium alloy, glass, pottery or plastics.Thisvacuum coating equipment 20 is provided with coating chamber 21.Saidalloy target material 23 is for being doped with the tungsten material of A, and wherein A can be one or more in molybdenum, niobium, the titanium; The atomic percentage conc of A is 4～12% in this electrochromic layer 13.Thisalloy target material 23 makes in the following manner: the configuration mixed powder, and to account for the total atom ratio of counting be 5-15% to A in this mixed powder, surplus is a tungsten; With above-mentioned mixed powder 1.0～20 * 105A base substrate is processed in hot pressing under the pressure of N, gets final product through 1700～2000 ℃ of sintering 1.5～3.0h.
Cleaning is to remove the spot onbase material 11 surfaces, and in the preferred embodiment of the present invention, thisbase material 11 is put into absolute ethyl alcohol and carried out ultrasonic cleaning, and scavenging period can be 5～10min.
Argon plasma is carried out on the surface of the base material after above-mentionedprocessing 11 clean, with the greasy dirt on furtherremoval base material 11 surfaces, and the adhesion that improvesbase material 11 surfaces and subsequentfilm.Base material 11 is put into thecoating chamber 21 of avacuum coating equipment 20, thiscoating chamber 21 is evacuated to 5.0～3.0 * 10-5Torr; Incoating chamber 21, feeding flow then is the argon gas (purity is 99.999%) of 200～400sccm (standard state ml/min); And apply-200～-300V be biased inbase material 11, argon plasma is carried out onbase material 11 surfaces cleans, scavenging period is 10～20min.
Adopt magnetron sputtering method at the saidelectrochromic layer 13 of deposition on the transparent conductive film of thebase material 11 after the argon plasma cleaning.
The power of saidalloy target material 23 can be 2.5～3.5kw; With oxygen is reacting gas, and the flow of oxygen is 50～75sccm, is working gas with the argon gas; The flow of argon gas is 300～400sccm; The bias voltage thatbase material 11 is applied is-100～-200V, heating the temperature that saidcoating chamber 21 makesbase material 11 is 300～400, the plated film time can be 30～60min.The thickness of saidelectrochromic layer 13 can be 500～800nm.
When thiselectrochromic layer 13 was applied the voltage of 2.1～2.8V, Li+ ion in the ionconductive layer 14 and electronics got in thiselectrochromic layer 13, and part tungsten is reduced into+5 valencys from+6 valencys, and thiselectrochromic layer 13 is by the colourless blueness that becomes.When removing extra electric field, said ion and electronics disappear, and tungsten is oxidized to+6 valencys from+5 valencys, and thiselectrochromic layer 13 is become colorless by blueness.
Come the preparation ofelectrochromic layer 13 of the present invention is specified through embodiment below.
Embodiment 1
The employedvacuum coating equipment 20 of present embodiment is the medium frequency magnetron sputtering coating machine, and company limited produces for south, Shenzhen innovation vacuum technique, and model is SM-1100H.
The material of the employedbase material 11 of present embodiment is a stainless steel; A is molybdenum and titanium in the saidalloy target material 23, and wherein the atomic percentage conc of molybdenum among the A and titanium is molybdenum 5% and titanium 5%, the tungsten powder body of surplus, and thisalloy target material 23 is processed through 1800 sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 10min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4kw, and the flow of oxygen is 60sccm, and the flow of argon gas is 300sccm, and bias voltage is-100V, and coating temperature is 250, and the plated film time is 60min.
Embodiment 2
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is an aluminium alloy; A is molybdenum, niobium and titanium in the saidalloy target material 23, and each atomic percentage conc of A is molybdenum 2%, niobium 1% and titanium 3%, the tungsten powder body of surplus, and thisalloy target material 23 is processed through 1850 sintering 1.5h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 10min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 3.5kw, and the flow of oxygen is 50sccm, and the flow of argon gas is 300sccm, and bias voltage is-150V, and coating temperature is 200 ℃, and the plated film time is 60min.
Embodiment 3
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is molybdenum, niobium and titanium in the saidalloy target material 23, and each atomic percentage conc of A is molybdenum 5%, niobium 2%, titanium 6%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1900 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 20min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 250 ℃, and the plated film time is 60min.
Embodiment 4
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a stainless steel; A is molybdenum, niobium and titanium in the saidalloy target material 23, and each atomic percentage conc of A is molybdenum 3%, niobium 3% and titanium 3%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1950 ℃ of sintering 1.5h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 10min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4.5kw, and the flow of oxygen is 60sccm, and the flow of argon gas is 300sccm, and bias voltage is-150V, and coating temperature is 200 ℃, and the plated film time is 45min.
Embodiment 5
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is molybdenum and niobium in the saidalloy target material 23, and each atomic percentage conc of A is molybdenum 5% and niobium 3%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1950 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Embodiment 6
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is a molybdenum in the saidalloy target material 23, and each atomic percentage conc of A is a molybdenum 15%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1900 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Embodiment 7
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is a niobium in the saidalloy target material 23, and each atomic percentage conc of A is a niobium 5%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1800 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 3.5kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Embodiment 8
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is a niobium in the saidalloy target material 23, and each atomic percentage conc of A is a niobium 15%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1950 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 4.5kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Embodiment 9
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is a titanium in the saidalloy target material 23, and each atomic percentage conc of A is a titanium 5%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1700 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 3kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Identical among the employedvacuum coating equipment 20 of present embodiment and the embodiment 1.
The material of the employedbase material 11 of present embodiment is a glass; A is a titanium in the saidalloy target material 23, and each atomic percentage conc of A is a titanium 15%, and surplus is a tungsten, and thisalloy target material 23 is processed through 1800 ℃ of sintering 2h through a base substrate is processed in mixed powder hot pressing.
Plasma clean: argon flow amount is 400sccm, and the bias voltage ofbase material 11 is-300V that the plasma clean time is 60min.
Sputter electrochromic layer 13: the power ofalloy target material 23 is 3.5kw, and the flow of oxygen is 65sccm, and the flow of argon gas is 300sccm, and bias voltage is-120V, and coating temperature is 150 ℃, and the plated film time is 60min.
Be appreciated that said firsttransparency conducting layer 12 can omit whenbase material 11 is processed by conductive material.
Preferred embodiments plated film spare 10 of the present invention is at the surfacedeposition electrochromic layer 13 ofbase material 11, and thisalloy target material 23 doping A have reduced the variable color voltage ofelectrochromic layer 13, make it have excellent more discoloration; And thiselectrochromic layer 13 has good reversibility, can improve the serviceable life of plated film spare 10 effectively.
In addition, those skilled in the art also can make various modifications, interpolation and the replacement on other form and the details in claim of the present invention scope of disclosure and spirit.Certainly, these all should be included within the present invention's scope required for protection according to the variations such as various modifications, interpolation and replacement that the present invention's spirit is made.
Claims (10)
1. a plated film spare comprises electrochromic layer, it is characterized in that: this electrochromic layer is the tungsten oxide layer that A mixes; Wherein A is one or more in molybdenum, niobium and the titanium; In this electrochromic layer, the A atomic percentage conc is 4～12%, and the variable color voltage of this electrochromic layer is 2.1～2.8V.
2. plated film spare as claimed in claim 1 is characterized in that: said electrochromism layer thickness is 500～800nm.
3. plated film spare as claimed in claim 1; It is characterized in that: said plated film spare also comprises the base material and first transparency conducting layer; Said first transparency conducting layer is formed on the base material, and said electrochromic layer is formed on first transparency conducting layer through the mode of magnetron sputtering.
4. electrochromic layer; It is characterized in that: this electrochromic layer is the tungsten oxide layer that A mixes, and wherein A is one or more in molybdenum, niobium and the titanium, in this electrochromic layer; The A atomic percentage conc is 4～12%, and the variable color voltage of this electrochromic layer is 2.1～2.8V.
5. the preparation method of a plated film spare may further comprise the steps:
The base material, vacuum coating equipment and the alloy target material that have transparency conducting layer are provided, and this alloy target material is the tungsten of doping A, and A is at least a in molybdenum, niobium and the titanium, and the A atomic percentage conc is 5～15%;
Base material and alloy target material are installed in the vacuum coating equipment;
Aerating oxygen, plated film forms electrochromic layer on base material, and the variable color voltage of this electrochromic layer is 2.1～2.8V.
6. the preparation method of plated film spare as claimed in claim 5 is characterized in that: this preparation method also is included in and before plated film, adopts argon gas that base material is carried out the step that plasma cleans.
7. the preparation method of plated film spare as claimed in claim 5; It is characterized in that: the technological parameter of said formation electrochromic layer is: the power of said alloy target material is 2.5～3.5kw, and the flow of oxygen is 50～75sccm, is working gas with the argon gas; The flow of argon gas is 300～400sccm; The bias voltage that base material is applied is-100～-200V, it is 300～400 ℃ that heating makes the temperature of said coating chamber, the plated film time is 30～60min.
8. the preparation method of plated film spare as claimed in claim 5 is characterized in that: the preparation of said alloy target material adopts following mode to realize: the mixed powder that said A powder and tungsten powder body form is 1.0～20 * 105The pressure of N, hot pressing are processed a base substrate, through 1700～2000 ℃ of sintering 1.5～3.0h.
9. the preparation method of plated film spare as claimed in claim 5 is characterized in that: said base material is stainless steel, aluminium alloy, magnesium alloy, glass, pottery or plastics.
10. the preparation method of plated film spare as claimed in claim 5 is characterized in that: the thickness of said electrochromic layer is 500～800nm.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100384845ACN102636931A (en) | 2011-02-15 | 2011-02-15 | Electro-chromic layer, coated element and preparation method of coated element |
| TW100105884ATW201234920A (en) | 2011-02-15 | 2011-02-22 | Electrochromic layer, coated article having same, and method for making the article |
| US13/166,323US20120206789A1 (en) | 2011-02-15 | 2011-06-22 | Coated article and method for making the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011100384845ACN102636931A (en) | 2011-02-15 | 2011-02-15 | Electro-chromic layer, coated element and preparation method of coated element |
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| CN2011100384845APendingCN102636931A (en) | 2011-02-15 | 2011-02-15 | Electro-chromic layer, coated element and preparation method of coated element |
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| Country | Link |
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| US (1) | US20120206789A1 (en) |
| CN (1) | CN102636931A (en) |
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Cited By (8)
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|---|---|---|---|---|
| CN103144380A (en)* | 2013-03-22 | 2013-06-12 | 中国南玻集团股份有限公司 | Three-silver light-adjusting glass |
| CN103145347A (en)* | 2013-03-22 | 2013-06-12 | 中国南玻集团股份有限公司 | Double-silver light-dimming glass |
| WO2015032200A1 (en)* | 2013-09-05 | 2015-03-12 | 华为技术有限公司 | All-solid-state electrochromic composite device and manufacturing method therefor |
| CN109154756A (en)* | 2016-07-07 | 2019-01-04 | 株式会社Lg化学 | Electrochromic device and method of manufacturing the same |
| CN111065758A (en)* | 2017-09-08 | 2020-04-24 | 依视路国际公司 | Durable electrochromic devices including tungsten oxide films prepared in high ion bombardment and low pressure deposition environments and methods of making the same |
| CN111286710A (en)* | 2020-03-30 | 2020-06-16 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass2O5Preparation method of multi-layer ion storage layer |
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| WO2015013631A2 (en)* | 2013-07-25 | 2015-01-29 | Hpo Assets Llc | Electrochromic films and related methods thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4009935A (en)* | 1975-07-11 | 1977-03-01 | Rca Corporation | Electrochromic device having a dopant therein to improve its color center absorption characteristics |
| CN1705045A (en)* | 2004-05-29 | 2005-12-07 | 李云平 | Technological process for preparing flexible conducting material by vacuum sputtering |
| US20070183066A1 (en)* | 1994-05-05 | 2007-08-09 | Donnelly Corporation | Signal mirror system for a vehicle |
| CN101188886A (en)* | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic all-solid-state electrochromic element and its preparation method |
- 2011
- 2011-02-15CNCN2011100384845Apatent/CN102636931A/enactivePending
- 2011-02-22TWTW100105884Apatent/TW201234920A/enunknown
- 2011-06-22USUS13/166,323patent/US20120206789A1/ennot_activeAbandoned
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4009935A (en)* | 1975-07-11 | 1977-03-01 | Rca Corporation | Electrochromic device having a dopant therein to improve its color center absorption characteristics |
| US20070183066A1 (en)* | 1994-05-05 | 2007-08-09 | Donnelly Corporation | Signal mirror system for a vehicle |
| CN1705045A (en)* | 2004-05-29 | 2005-12-07 | 李云平 | Technological process for preparing flexible conducting material by vacuum sputtering |
| CN101188886A (en)* | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic all-solid-state electrochromic element and its preparation method |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145347A (en)* | 2013-03-22 | 2013-06-12 | 中国南玻集团股份有限公司 | Double-silver light-dimming glass |
| CN103144380B (en)* | 2013-03-22 | 2016-08-03 | 中国南玻集团股份有限公司 | Three silver medal dimming glass |
| CN103145347B (en)* | 2013-03-22 | 2016-12-28 | 中国南玻集团股份有限公司 | Double silver dimming glass |
| CN103144380A (en)* | 2013-03-22 | 2013-06-12 | 中国南玻集团股份有限公司 | Three-silver light-adjusting glass |
| WO2015032200A1 (en)* | 2013-09-05 | 2015-03-12 | 华为技术有限公司 | All-solid-state electrochromic composite device and manufacturing method therefor |
| CN104423114A (en)* | 2013-09-05 | 2015-03-18 | 华为技术有限公司 | All-solid-state electrochromic multiple device and preparation method thereof |
| CN104423114B (en)* | 2013-09-05 | 2018-03-06 | 华为技术有限公司 | A kind of full-solid electrochromic multiple device and preparation method thereof |
| CN109154756B (en)* | 2016-07-07 | 2021-04-27 | 株式会社Lg化学 | Electrochromic device and method of making the same |
| CN109154756A (en)* | 2016-07-07 | 2019-01-04 | 株式会社Lg化学 | Electrochromic device and method of manufacturing the same |
| CN111065758A (en)* | 2017-09-08 | 2020-04-24 | 依视路国际公司 | Durable electrochromic devices including tungsten oxide films prepared in high ion bombardment and low pressure deposition environments and methods of making the same |
| CN111065758B (en)* | 2017-09-08 | 2022-06-21 | 依视路国际公司 | Durable electrochromic devices including tungsten oxide films prepared in high ion bombardment and low pressure deposition environments and methods of making the same |
| CN111286710A (en)* | 2020-03-30 | 2020-06-16 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass2O5Preparation method of multi-layer ion storage layer |
| CN111286710B (en)* | 2020-03-30 | 2022-08-05 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass 2 O 5 Preparation method of multi-layer ion storage layer |
| CN113759624A (en)* | 2021-09-09 | 2021-12-07 | 宁波伯宇科技有限公司 | A process for manufacturing curved electrochromic lenses |
| CN113759624B (en)* | 2021-09-09 | 2024-11-05 | 苏州伯宇科技有限公司 | A process for manufacturing curved electrochromic lenses |
| CN116445872A (en)* | 2023-04-19 | 2023-07-18 | 合肥工业大学 | An amorphous molybdenum-doped tungsten oxide electrochromic material and its preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201234920A (en) | 2012-08-16 |
| US20120206789A1 (en) | 2012-08-16 |
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